High pressure parallel reactor

ABSTRACT

A method for reacting a plurality of materials in parallel within a reactor vessel having a plurality of reaction wells formed therein. Each of the reaction wells has an open end exposed to a common pressure chamber defined by the reactor vessel. The method includes opening a cover of the reactor vessel, inserting components into the reaction wells, closing the cover of the reactor vessel to create a sealed chamber, supplying a gas substantially above atmospheric pressure that reacts with the components within the reaction wells, and releasing pressure from the reactor vessel.

RELATED APPLICATION

This patent application is a divisional of U.S. patent application Ser.No. 09/619,416, filed Jul. 19, 2000 now U.S. Pat. No. 7,018,589, whichis incorporated herein by reference in its entirety.

FIELD OF THE INVENTION

The present invention relates generally to parallel batch reactors, andmore particularly, to high pressure reactors for parallel synthesis andscreening of materials.

BACKGROUND OF THE INVENTION

The discovery of new materials with novel chemical and physicalproperties often leads to the development of new and usefultechnologies. The discovery of new materials depends largely on theability to synthesize and analyze new compounds. Scientists are thus,always searching for a more efficient, economical, and systematicapproach for the synthesis of novel materials. Combinatorialtechnologies are often used to accelerate the speed of research,maximize the opportunity for breakthroughs, and expand the amount ofavailable information. Combinatorial chemistry involves synthesizingmicroscale quantities of a compound and then testing thousands ofcompounds quickly.

The use of combinatorial technologies allows high density libraries ofvery large numbers of materials to be created using parallel synthesis.High throughput screens are then used to test these materials fordesired properties to identify potential optimized compounds.Combinatorial technologies may be used to optimize and validate manyvariations of a material, formulation, or microdevice. Variables such astemperature, pressure, atmosphere, and concentration can be quicklyadjusted and tested in a single experiment.

In parallel synthesis, different compounds are synthesized in separatevessels, often in an automated fashion. A commonly used format forparallel synthesis is a multi-well microtiter plate. Roboticinstrumentation can be used to add different reagents or catalysts toindividual wells of a microtiter plate in a predefined manner to producecombinatorial libraries. Devices have been developed for automatingcombinatorial parallel synthesis. One such device includes reactionblocks containing multiple reaction vessels each individually sealed.These devices often require substantial sealing arrangements and do notprovide means for pressurizing the individual vessels. Other devicessupply an inert gas to a plurality of reactor vessels, however, the gasis only supplied at one or two psi above atmospheric pressure to controlthe environment during the reaction. These devices are not designed towithstand high pressure operation.

SUMMARY OF THE INVENTION

An apparatus and method for synthesis and screening of materials aredisclosed.

A method for reacting a plurality of materials in parallel with areactor vessel having a plurality of reaction wells formed in a base ofthe vessel, each of the reaction wells having an open end exposed to acommon pressure chamber defined by the reactor vessel, generallycomprises: opening a cover of the reactor vessel; inserting componentsinto the reaction wells; closing the cover of the reactor vessel tocreate a sealed chamber; and supplying a gas substantially aboveatmospheric pressure that reacts with the components within the reactionwells.

The above is a brief description of some deficiencies in the prior artand advantages of the present invention. Other features, advantages, andembodiments of the invention will be apparent to those skilled in theart from the following description, drawings, and claims.

BRIEF DESCRIPTION OF THE DRAWINGS

FIG. 1 is an exploded view of a reactor vessel of the present invention.

FIG. 2 is a perspective of the reactor vessel of FIG. 1.

FIG. 3 is a plan view of the reactor vessel of FIG. 1

FIG. 4 is a side view of the reactor vessel of FIG. 1.

FIG. 5 is a front view of the reactor vessel of FIG. 1.

FIG. 6 is a plan view of the reactor vessel of FIG. 1 with internalparts of the vessel shown in phantom.

FIG. 7 is a cross-sectional view of the vessel taken in the planeincluding line 7—7 of FIG. 6.

FIG. 8 is a cross-sectional view of the vessel taken in the planeincluding line 8—8 of FIG. 6.

FIG. 9 is a cross-sectional view of the vessel taken in the planeincluding line 8—8 of FIG. 6 with coil springs disposed at a closedbottom of reaction wells to force vials within the wells upward againsta cover plate.

FIG. 10 is a flowchart illustrating a process utilizing the reactorvessel of FIG. 1.

FIG. 11 is a perspective of a second embodiment of a reactor vessel ofthe present invention.

FIG. 12 is a perspective of the reactor vessel of FIG. 11 in an openposition.

FIG. 13 is a cross-sectional view of the reactor vessel of FIG. 11.

FIG. 14 is a partial cross-sectional view of the vessel of FIG. 1 with acheck valve inserted as a flow restriction device.

Corresponding reference characters indicate corresponding partsthroughout the several views of the drawings.

DETAILED DESCRIPTION OF THE INVENTION

The following description is presented to enable one of ordinary skillin the art to make and use the invention. Descriptions of specificembodiments and applications are provided only as examples and variousmodifications will be readily apparent to those skilled in the art. Thegeneral principles described herein may be applied to other embodimentsand applications without departing from the scope of the invention.Thus, the present invention is not to be limited to the embodimentsshown, but is to be accorded the widest scope consistent with theprinciples and features described herein. For purpose of clarity,details relating to technical material that is known in the technicalfields related to the invention have not been described in detail.

Referring now to the drawings, and first to FIGS. 1–6, an apparatus ofthe present invention is shown and generally indicated at 20. Theapparatus 20 comprises a reactor vessel defining a pressure chamber 26and a plurality of reaction wells 30 internal to the reactor vessel andexposed to the pressure chamber. The pressure chamber 26 is pressurizedwith an inert gas to pressurize components within the reaction wells ora gas selected to react with components within the reaction wells. Thecommon pressurization area defined by the pressure chamber 26 simplifiesthe sealing required as compared to individually sealed reaction wellsof conventional devices. Furthermore, the common pressure chamber 26exposes each reaction well 30 to generally the same pressure, whereasindividually pressurized reaction wells are often exposed to varyingpressures due to leaks or uneven filling (when heated), which introducesundesirable variability into the testing.

The apparatus 20 may be used to perform parallel synthesis or screeningof materials or other experimentation involving reactions of multiplecomponents. For example, the apparatus 20 may be utilized for reactionswhere one or more components is a gas such as hydrogenations,carbonilations, oxidations and polymerizations with gaseous monomers.The apparatus may also be used with homogeneous, chiral, orheterogeneous catalysts (i.e., catalysts which enable catalyticreactions to occur with the reactants and catalysts residing indifferent phases (e.g., solid/liquid, solid/gas, liquid/gas)), orpolyolefin and butyl rubber polymerizations. It is to be understood thatthe applications described herein are merely examples of uses of theapparatus 20 and methods of the present invention and that the apparatusmay be used for other applications without departing from the scope ofthe invention.

As shown in FIGS. 1–3, the reactor vessel has an overall rectangularshape and comprises two sections; a base member 32 and a top member (orcover) 34 (FIGS. 1 and 2). The combination of the base 32 and cover 34form a manifold generally in the form of a rectangular parallelepiped.Internal surfaces of the base 32 and cover 34 define an internal cavitywhich forms the pressure chamber 26 (FIGS. 7 and 8). The pressurechamber may have a volume of approximately ten cubic inches, forexample. The base member 32 includes a bottom 40, a pair of opposingside walls 42, and a pair of opposing end walls 44 (FIGS. 4 and 5). Thecover 34 includes a periphery flange 48 configured to mate with aperiphery flange 50 extending from the walls 42, 44 of the base member32 (FIGS. 1 and 2). The flanges 48, 50 of the cover 34 and base 32include a plurality of openings 52 (ten shown) for receiving bolts 54,screws, or other fasteners. The base 32 and cover 34 may also beattached by other suitable attachment means such as external clamps. Thebase 32 includes a groove 58 extending around a periphery thereof forreceiving a sealing gasket 60 (FIGS. 1, 7 and 8). The gasket 60 isinterposed between the base 32 and cover 34 to provide a sealtherebetween. The groove 58 for the gasket 60 may be machined intoeither a bottom surface of flange 48 of the cover 34, or a top surfaceof flange 50 of the base 32. The gasket 60 may be an o-ring formed fromPTFE, neoprene, butyl rubber, Teflon coated elastomer, Viton, expandedTeflon, graphite, or Kalrez, for example.

The reactor vessel includes an inlet port 70 in fluid communication withthe pressure chamber 26 (FIGS. 2 and 6). A quick release fitting 72 ispreferably coupled to the inlet port 70 for attaching the port to aflexible hose or rigid tube (not shown) connected to a pressure supplydevice. The flexible hose or rigid gas supply tube may also be leftconnected and the fill valve open during an experiment. If a vacuum isto be applied to the chamber 26, a vacuum supply device may also beattached to the pressure port 70 or another inlet port on the reactorvessel. A fill valve 74 is attached to the inlet port to control theapplication of pressure to the vessel. The fill valve 74 may have amanual or electronic pressure control valve. A pressure sensor (notshown) may be inserted inline with the fill valve 74 or inserted intothe pressure chamber 26 or one or more of the reaction wells 30 tomonitor the pressure within the vessel. The inlet supply system mayallow for a series of purging, venting, or pressurization cycles, withone or more gases or with vacuum without disconnecting the supply lines.The pressure source may be an inert gas such as nitrogen, argon, helium,carbon dioxide, or air, or a reactive gas such as hydrogen, oxygen,hydrogen chloride, or ammonia. Mixtures of gases may also be used. Thereactor vessel further includes an opening for a pressure release valve78 to prevent over pressurization of the vessel.

The base 32 and cover 34 may be formed from aluminum, titanium, steel,or any other suitable material. The material of the reactor vessel ispreferably selected to be chemically inert to the reaction of interestand allow the vessel to operate at high temperature (e.g., 150–250° C.)and high pressure (10–1000 psig). For example, if the apparatus is to beoperated at 290 psig and 150° C. (for e.g., gaseous monomer or reagentuse), 6061-T6 aluminum, which has been hard anodized, may be used. Ifthe operating pressure is 1000 psig and operating temperature is 200°C., the material may be 17-4PH, H1100 stainless steel or 6Al-4Vtitanium. For some applications, the stainless steel or other materialmay be coated or surface treated. It is to be understood that thetemperature or pressure applied to the reactor vessel or the materialsused to form the base 32 and cover 34 may be different than describedherein without departing from the scope of the invention. The reactorvessel is preferably designed to withstand pressures substantially aboveatmospheric pressure (i.e., 14.7 psi). The vessel is preferably designedto withstand pressures above 10 psig, and more preferably pressuresabove 50 psig. The vessel may also be designed, for example, to operateat pressures of 15 psig, 20 psig, 30 psig, 40 psig, 100 psig, 300 psig,500 psig, 1000 psig, or other selected pressures. The vessel ispreferably designed to withstand temperatures up to 200° C., but mayalso be designed to operate at 250° C., 315° C., or higher temperatures.

The reaction wells 30 are preferably integrally formed within the basemember 32 or another member coupled to the base member. As shown inFIGS. 7 and 8, the wells 30 are machined into an upper planar surface 80of the base member 32. The wells 30 are preferably machined as close aspossible to one another. Similarly, a bottom surface 84 of the well 30is left with sufficient material to withstand pressures applied to thewells. The base member 32 may also serve as a temperature control meansfor controlling the reaction temperature in the reaction wells 30, inwhich case the bottom surface 84 of the reaction wells 30 is sized toprovide the required conductivity between an external heat source, suchas a heating plate on which the reaction vessel is placed, and thereaction wells. The reactor vessel may be placed, for example, on atemperature control plate which is contiguous to the lower surface ofthe reactor vessel for the transfer of thermal energy therebetween. Thethermal control plate may be a plate formed of thermally conductivematerial with passages for conveying a heating or cooling fluid throughthe plate, or other heat generating device, as is well known by thoseskilled in the art. If the reactor vessel is designed for heatingcomponents within the reaction wells, the manifold is preferably formedfrom a thermally conductive material, such as an aluminum alloy. Thereactor vessel may also be placed in an oven to heat the componentswithin the reaction wells 30.

The reaction wells 30 may also be formed within a block separate fromthe base of the reactor vessel. For example, the reaction wells may beformed within a metal, nylon, Teflon, or other polymer material block.The block may be a microtiter plate, as described below.

The reaction vessel is preferably configured to correspond to a standardmicrotiter plate format. The microtiter plate is a widely used means forhandling, processing, and analyzing large numbers of small samples inthe biochemistry and biotechnology fields. Typically, a microtiter plateis approximately 3.4 inches wide and 5.0 inches long and contains 96identical sample wells in an 8 by 12 rectangular array on 9 millimetercenters. A wide variety of equipment is available for automatichandling, processing, and analyzing of samples in this microtiter plateformat. It is to be understood that depending upon the scale of theapparatus, the block may contain a greater or fewer number of reactionwells of various geometries arranged in any configuration.

In the embodiment shown in FIGS. 1–8, the base includes 96 reactionwells 30 in an 8 by 12 array, corresponding to the standard microtiterplate format used in industry for high throughput screening of compoundsand biological assays. In preferred embodiments, the number of testwells is equal to 96×N, where N is an integer ranging from 1–100,preferably 1–10, and more preferably 1–5. The outside dimensions of thevessel preferably correspond to the standard microtiter format (e.g.,approximately 5.0 inches long (l), 3.4 inches wide (w), and 0.5–2.0inches high (h) (FIGS. 4 and 5). For example, the reactor vessel mayhave a length (l) of 5.030 inches, a width (w) of 3.365 inches andheight (h) of 2.175 inches. It is to be understood that the reactorvessel may have external dimensions different than the standardmicrotiter plate format or have a different number or arrangement ofreaction wells 30 without departing from the scope of the invention. Forexample, the reactor may have a 3 by 4 array of reaction wells, eachwell having a fluid volume of approximately 16 milliliters. Otherarrays, such as a 3 by 5 array or a 100 by 100 array may also be used.

Components used in the synthesis or screening may be added directly tothe reaction wells 30 or the reaction wells 30 may be lined with aninert liner to prevent reactions between chemicals and the base member.As shown in FIGS. 7 and 8, vials 90 may be inserted into the wells 30for receiving the components. The vials 90 may be formed from glass orother suitable materials. The vials 90 preferably extend above thereaction well openings formed in the base member 32. The glass vials 90may have an internal volume of approximately 2 milliliters, for example.

A flow restriction device 92 is preferably placed over the reactionwells 30 to reduce vapor phase cross-talk between adjacent wells 30(FIGS. 7 and 8). The flow restriction device 92 may comprise, forexample, a cover member having a plurality of very small vent holes 96aligned with the reaction wells 30 to provide fluid communicationbetween the wells and the pressure chamber 26. The cover member 92 maybe a rigid metal plate with vent holes drilled therein or a flexibleelastomeric sheet (e.g., septum sheet) with vent holes punched therein.The member 92 may also be a porous sheet with the pores providing fluidcommunication between the reaction wells 30 and the pressure chamber 26.The flow restriction device 92 may also include check valves 140 whichallow flow into the reaction wells 30 but restrict flow from thereaction wells to the pressure chamber 26 (shown schematically in FIG.14). The vent holes within the flow restriction device 92 may also bemicromachined flow restrictions.

A coil spring 95 (or elastomeric material) may be placed at the bottomof each of the reaction wells to force the vials upward and bias theopen ends of the vials against the flow restriction device 92, as shownin FIG. 9. The flow restriction device 92 is preferably removablyattached to the base member with bolts 98 or other suitable attachmentmeans. The flow restriction device 92 may also be coupled or integrallyformed with the cover 34 so that the device is automatically disposedadjacent to the open ends of the reaction wells 30 when the cover ismated with the base member 32 and closed.

The materials of the base member 32, cover 34, flow restriction device92, gasket 60, and vials 90 are preferably selected to be chemicallysuitable for the application (i.e., will not be attacked, solubilized,softened, or otherwise interact with the reagents, solvents, solids,products, or other components which are either added to the vessel orproduced during a reaction sequence). The materials are also preferablychosen to assure that reactant, products, or by-products of the reactionare not adsorbed or otherwise trapped by the materials.

FIG. 10 is a flowchart illustrating a process for utilizing theapparatus 20 of the present invention. At step 100, the cover 34 isremoved from the base member 32 (or placed in an open position) to allowaccess to the interior of the reactor vessel (FIGS. 1 and 10). If thereaction wells are not formed in the base member, the block containingthe reaction wells is positioned within the base member 32. Thecomponents to be tested are then placed within the reaction wells 30(step 102). Preferably, the composition of the materials placed withineach of the wells 30 varies from one reaction well to the next. Thecover plate 92 is then placed over the base member 32 with fasteneropenings within the plate aligned with openings formed in the base (orreaction well block) (step 104). Bolts 98 or other suitable fasteners,are inserted into the aligned openings to attach the cover plate 92 tothe base member 32. The cover 34 is then attached to the base 32 withbolts 54 or other fasteners (step 106). A supply line (not shown) isconnected to the quick release coupling 72 at the inlet port 70 and thefill valve 74 is opened until the required pressure is reached withinthe pressure chamber 26 (step 108) (FIGS. 6 and 10). The gas supplied tothe vessel may be an inert gas or a gas that reacts with the componentsplaced into the reaction wells 30.

After the pressurized gas is added to the vessel and the pressurechamber 26 has reached the appropriate operating pressure, the fillvalve 74 is closed, the supply line is removed, and the entire assemblyis inserted into an oven or placed on a heating plate (steps 110 and112). Agitation of components within the reaction wells 30 may beachieved by shaking or magnetic stirring. For example, the apparatus maybe placed on an oven/shaker assembly or a magnetic stirrer may be usedto mix the reactants. The base 32 and cover 34 are preferably aluminumor titanium if magnetic stirring is used. Once the reaction is complete,pressure is removed from the pressure chamber 26 through the fill valve74 or an outlet or vent within the housing (step 116). The cover 34 isopened and the cover plate 92 is removed from the base member 32 (step118). If vials 90 are used, the vials are removed from the reactionwells 30 for analysis or their contents are sampled (step 120). If thematerials are placed directly into the reaction wells 30, a pipette orother suitable tool may be used to remove contents of the wells. Thecontents of the reaction wells 30 are then analyzed by techniques wellknown by those skilled in the art.

FIGS. 11–13 show a second embodiment of a reactor vessel of the presentinvention, generally indicated at 200. The reactor vessel 200 includes apressure chamber 202 sized for receiving a microtiter plate 205. Thepressure chamber 202 may be formed from 6061-T6 aluminum, or any othersuitable material. The vessel 200 includes a fill valve 208 and pressurerelief valve 210 in communication with the pressure chamber 202. Thevessel 200 further includes a door 204 movable between an open position(shown in FIG. 12) for inserting the microtiter plate 205 and a closedposition (shown in FIG. 11) for creating a sealed pressure chamber. Aquick-operating fastening device is used to move the door 204 to itsclosed position and sealingly engage the door with the pressure chamber202. The door 204 may be formed from stainless steel or other suitablematerials. The door 204 includes two pin receiving openings 211 formedin a top surface of the door and extending longitudinally through aportion of the door (FIG. 12). The openings 211 are sized for receivingdoor latching pins 212 which extend downwardly from latch mechanism 214.The latch mechanism 214 is coupled to a handle 216 for movementtherewith. The latch mechanism 214 and handle 216 each include a pair oflegs 218, 220, respectively. The legs 218 of the latch mechanism 214 arespaced apart such that each leg is positioned adjacent to an innersurface of the legs 220 of the handle 216. The legs 218, 220 areattached by bolts or other suitable attachment means to create a fourbar mechanism. The door 204 may also be coupled to the handle 216 sothat the door rotates towards its closed position as the handle isrotated upwardly.

When the handle 216 is in its open position the latching mechanism 214is in a raised positioned (FIG. 12). As the handle 216 is rotatedupwardly it pulls the door latching mechanism 214 downwardly along alinear axis and forces the pins 212 into the pin receiving openings 211within the door 204 as the door is rotated upwardly by the handle (FIG.11). The handle 216 includes latching members 224 attached to the legs220 thereof to lock the door 204 in its closed position. When the door204 is in its closed position, an inner surface 226 of the door is insealing engagement with and an o-ring 230 positioned within a grooveextending around the periphery of the opening in the pressure chamber202. A spring loaded clamping device 240 is positioned adjacent to theend of the plate 205 opposite the door 204 to hold the plate in place.The quick-operating fastening device allows for quick and easy openingand closing of the vessel without the need to loosen or tighten bolts orother attachment means.

The entire assembly 200 may be placed into an oven or on an orbitalshaker. As shown and described above, the vessel 200 is compact since itis sized specifically for receiving a microtiter plate. For example, thevessel 200 may have a length (L) of 7.625 inches. It is to be understoodthat the vessel may have different configurations than shown anddescribed herein without departing from the scope of the invention. Forexample, the vessel 200 may be sized for receiving more than onemicrotiter plate or have a quick release mechanism different than shown.

The following examples illustrate principles and advantages of theinvention.

EXAMPLE 1 Heterogeneous Catalysis

The reaction vessel used for this experiment was formed from 6061-T6aluminum and had 96 reaction wells. The following components were firstadded to a 4 ml glass vial to form a solution:

10.9 mg of 1% palladium on activated carbon;

3.090 ml ethyl alcohol; and

0.020 ml nitrobenzene.

The vial was shaken by hand and then placed on a stir plate to mix usinga magnetic micro-stir bar within the vial. Samples containing 0.377 mlof the solution were pipetted into two of the 96 wells. The reactor wasthen sealed with an o-ring and the cover was placed over the base of thereactor. Bolts were inserted into the aligned openings of the base andcover and each torqued to 10 ft-lbs. A gas supply line was attached tothe reactor vessel and the vessel was pressurized and vented three timesto remove the air inside. The vessel was then pressurized to 30 psigwith pure hydrogen gas. The fill valve was closed and the gas linedisconnected before placing the apparatus in a mixing oven. The reactorwas heated at 30° C. for one hour while mixing. The vessel was thenvented and opened. Thin layer chromatography (TLC) and high pressureliquid chromatography (HPLC) were performed and showed that thenitrobenzene in both wells was fully converted and only the desiredproduct, aniline, was detected.

EXAMPLE 2 Cross-Talk

In the following example, two aluminum reactor vessels each having 96reaction wells were used. One of the reactor vessels included a septumsheet (flow restriction device) having punctured holes aligned with eachof the reaction wells. The other reactor vessel did not include a flowrestriction device to reduce cross talk between reaction wells. Blanksof pure toluene were placed in eight reaction wells within each of thereactors. The remaining reaction wells contained a mixture of heptane,toluene, and octene. Nitrogen gas was supplied to each of the reactorvessels at an initial pressure of 160 psig and temperature of 25° C. Thefinal pressure within the vessels was 260 psig after 45 minutes in anoven at 200° C. The following are the gas chromatography (GC) testresults:

-   The original mix before the test included the following components:    -   43.47% heptane, 49.03% toluene, and 7.50% octene.-   The original toluene blank before the test contained:    -   0.05% (in heptane position), 99.93% toluene, and 0.02% (in        octene position).-   The average composition of the mix (with flow restriction device)    after the test was:    -   41.51% heptane, 51.35% toluene, and 7.14% octene.-   The average composition of the mix (without flow restriction device)    after the test was:    -   41.82% heptane, 50.50% toluene, and 7.68% octene.        Thus, some vapor was being transported out of the reaction wells        in both reactor vessels.

The average composition of the toluene blanks (with flow restrictiondevice) after the test was:

-   -   0.47% heptane, 99.49% toluene, and 0.04% octene.

-   The average composition of the toluene blanks (without flow    restriction device) after the test was:    -   17.11% heptane, 81.26% toluene, and 1.68% octene.        Thus, the flow restriction device helped to prevent vapor        transport (cross-talk) into the wells.

As can be observed from the foregoing, the apparatus 20, 200 and methodof the present invention have numerous advantages. The reaction wells 30are all exposed to a common pressure chamber 26 which results insimplification of the apparatus, reduced variation betweenpressurization of the reaction wells, and reduced manufacturing andprocessing costs. The apparatus is well suited for auxiliary processesincluding heating, shaking, and robotic automation. Furthermore, sincethere is a fewer number of sealed volumes (e.g., one versus ninety-six)the apparatus provides increased reliability and easier maintenance. Thedesign of the reactor vessel allows for pressurization of the reactionwells with a pressurized gas at a pressure substantially aboveatmospheric pressure.

Although the present invention has been described in accordance with theembodiments shown, one of ordinary skill in the art will readilyrecognize that there could be variations made to the embodiments withoutdeparting from the scope of the present invention. Accordingly, it isintended that all matter contained in the above description and shown inthe accompanying drawings shall be interpreted as illustrative and notin a limiting sense.

1. A method for reacting a plurality of materials in parallel within abatch reactor vessel having a plurality of reaction wells formedtherein, each of said plurality of reaction wells having a gasimpermeable closed end and an open end exposed to a common pressurechamber defined by the reactor vessel, the method comprising: opening acover of the reactor vessel; inserting components into the reactionwells; closing the cover of the batch reactor vessel to create afluidically sealed chamber; supplying a gas at a pressure substantiallyabove atmospheric pressure and below or at 1000 psig, that reacts withthe components within the reaction wells; and releasing pressure fromthe reactor vessel.
 2. The method of claim 1 further comprising coveringa portion of the open ends of the reaction wells to reduce vapor phasecross-talk between the reaction wells.
 3. The method of claim 1 furthercomprising, after inserting said components into the reactions wells,placing a flow restriction device over said reaction wells such that theflow restriction device is interposed between the reaction wells andsaid common pressure chamber when the cover of the reactor vessel isclosed.
 4. The method of claim 3 wherein the flow restriction devicecomprises a plurality of vent holes formed therein and aligned with saidplurality of reaction wells.
 5. The method of claim 4 wherein each ofsaid vent holes has a diameter substantially smaller than a diameter ofthe aligned reaction well.
 6. The method of claim 4 wherein saidplurality of vent holes comprises a plurality of micromachined holes. 7.The method of claim 3 wherein the flow restriction device comprises aplurality of check valves configured to allow flow into the reactionwells and restrict flow from the reaction wells into said commonpressure chamber.
 8. The method of claim 1 further comprisingrestricting flow from said plurality of reaction wells to reducecross-talk between said plurality of reaction wells.
 9. The method ofclaim 1 further comprising inserting a microtiter plate into saidreactor vessel, said plurality of reaction wells formed in themicrotiter plate.
 10. The method of claim 1 further comprising openingthe cover of the reactor vessel and removing said components from saidopen ends of the reaction wells.
 11. The method of claim 1 furthercomprising heating said cpmponents inserted in the reaction wells. 12.The method of claim 11 further comprising stopping said supply of gasbefore heating said components.
 13. The method of claim 1 furthercomprising: covering a portion of the open ends of the reaction wells toreduce vapor phase cross-talk between the reaction wells; andrestricting flow from said plurality of reaction wells into said commonpressure chamber.
 14. The method of claim 1 further comprising removingsaid gas supply while maintaining pressure in the reactor vessel.
 15. Amethod for reacting a plurality of materials in parallel within a batchreactor vessel having a plurality of reaction wells formed therein, eachof said plurality of reaction wells having a gas impermeable closed endand an open end exposed to a common pressure chamber defined by thereactor vessel, the method comprising: opening a cover of the reactorvessel; inserting components into the reaction wells; closing the coverof the batch reactor vessel to create a fluidically sealed chamber;supplying a gas at a pressure between approximately 100 psig and 1000psig that reacts with the components within the reaction wells; andreleasing pressure from the reactor vessel.
 16. The method of claim 15further comprising: covering a portion of the open ends of the reactionwells to reduce vapor phase cross-talk between the reaction wells; andrestricting flow from said plurality of reaction wells into said commonpressure chamber.
 17. The method of claim 15 further comprising removingsaid gas supply while maintaining pressure in the reactor vessel.
 18. Amethod for reacting a plurality of materials in parallel within a batchreactor vessel having a plurality of reaction wells formed therein, eachof said plurality of reaction wells having a gas impermeable closed endand an open end exposed to a common pressure chamber defined by thereactor vessel, the method comprising: opening a cover of the reactorvessel; inserting components into the reaction wells; placing a flowrestriction plate over said reaction wells such that the flowrestriction plate is interposed between the reaction wells and saidcommon pressure chamber when the cover of the batch reactor vessel isclosed; closing the cover of the batch reactor vessel to create afluidically sealed chamber; supplying a gas substantially aboveatmospheric pressure that reacts with the components within the reactionwells; and releasing pressure from the reactor vessel; wherein the flowrestriction plate comprises a plurality of check valves movable betweena first position wherein flow is allowed from said common pressurechamber into the reaction wells and a second position wherein flow isrestricted from the reaction wells into said common pressure chamber.19. The method of claim 18 further comprising inserting a microtiterplate into said reactor vessel, said plurality of reaction wells formedin the microtiter plate.
 20. The method of claim 18 further comprisingmixing said components inserted in the reaction wells.